#------------------------------------------------------------------------------ #$Date: 2020-04-25 01:18:02 +0300 (Sat, 25 Apr 2020) $ #$Revision: 251163 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557906.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557906 loop_ _publ_author_name 'Itami, Kenichiro' 'Okude, Ryo' 'Mori, Genki' 'Yagi, Akiko' _publ_section_title ; Programmable Synthesis of Multiply Arylated Cubanes through C-H Metalation and Arylation ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC01909G _journal_year 2020 _chemical_absolute_configuration unk _chemical_formula_sum 'C31 H39 N3 O2' _chemical_formula_weight 485.65 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-04-24 downloaded from the CCDC. ; _cell_angle_alpha 113.955(2) _cell_angle_beta 97.7538(17) _cell_angle_gamma 91.349(2) _cell_formula_units_Z 2 _cell_length_a 8.9740(2) _cell_length_b 11.7370(3) _cell_length_c 14.0121(3) _cell_measurement_reflns_used 10951 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 30.5110 _cell_measurement_theta_min 2.9030 _cell_volume 1331.40(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 14591 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.299 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.211 _exptl_crystal_description block _exptl_crystal_F_000 524 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.267 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.036 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 4665 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0365 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.6107P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.0949 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4210 _reflns_number_total 4665 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01909g2.cif _cod_data_source_block 2p _cod_database_code 1557906 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.981 _shelx_estimated_absorpt_t_max 0.992 _shelx_res_file ; TITL qq qq.res created by SHELXL-2016/6 at 20:10:36 on 13-Nov-2018 REM Yadorkari-X generated CELL 0.71073 8.9740 11.7370 14.0121 113.9550 97.7538 91.3490 ZERR 2.0 0.0002 0.0003 0.0003 0.0020 0.0017 0.0020 LATT 1 REM SPGR P-1 triclinic SFAC C H N O UNIT 62 78 6 4 SIZE 0.25 0.20 0.10 TEMP -150.0 L.S. 4 FMAP 2 PLAN -25 ACTA CONF LIST 4 WPDB -1 BOND $H MERG 2 OMIT -10.000000 50.000000 WGHT 0.040500 0.610700 FVAR 3.21919 O1 4 0.210845 0.174535 0.316877 11.00000 0.01844 0.02899 = 0.01914 0.01010 0.00057 -0.00044 C1 1 0.327436 0.200778 0.381593 11.00000 0.01859 0.01454 = 0.01812 0.00603 0.00305 0.00109 N1 3 0.465528 0.213334 0.356560 11.00000 0.01837 0.02269 = 0.01724 0.00820 0.00464 -0.00026 C2 1 0.606437 0.234493 0.430975 11.00000 0.01649 0.02723 = 0.02259 0.01118 0.00399 0.00048 AFIX 13 H12 2 0.579207 0.226704 0.495089 11.00000 -1.20000 AFIX 0 C3 1 0.714765 0.135097 0.384749 11.00000 0.02449 0.03545 = 0.04041 0.01994 0.01119 0.00849 AFIX 137 H16 2 0.660862 0.051744 0.357021 11.00000 -1.50000 H17 2 0.798537 0.142536 0.440184 11.00000 -1.50000 H18 2 0.754367 0.147270 0.327398 11.00000 -1.50000 AFIX 0 C4 1 0.681767 0.366072 0.466888 11.00000 0.02279 0.03080 = 0.03283 0.00993 0.00234 -0.00397 AFIX 137 H19 2 0.705912 0.378201 0.405311 11.00000 -1.50000 H20 2 0.774825 0.376969 0.516316 11.00000 -1.50000 H21 2 0.612999 0.427646 0.502128 11.00000 -1.50000 AFIX 0 C5 1 0.478066 0.207176 0.250051 11.00000 0.02596 0.03276 = 0.01949 0.01097 0.00807 -0.00180 AFIX 13 H13 2 0.587262 0.226927 0.250581 11.00000 -1.20000 AFIX 0 C6 1 0.393642 0.306664 0.228263 11.00000 0.04044 0.04735 = 0.03642 0.02943 0.00692 -0.00010 AFIX 137 H22 2 0.284830 0.287329 0.221296 11.00000 -1.50000 H23 2 0.416954 0.308422 0.162506 11.00000 -1.50000 H24 2 0.424583 0.388538 0.286905 11.00000 -1.50000 AFIX 0 C7 1 0.434432 0.075733 0.163511 11.00000 0.04408 0.04267 = 0.02120 0.00248 0.01122 -0.00167 AFIX 137 H25 2 0.495442 0.016136 0.180227 11.00000 -1.50000 H26 2 0.452549 0.073978 0.095524 11.00000 -1.50000 H27 2 0.327279 0.052664 0.159199 11.00000 -1.50000 AFIX 0 C8 1 0.314201 0.217087 0.492304 11.00000 0.01425 0.01750 = 0.01761 0.00638 0.00234 0.00091 C9 1 0.155466 0.229798 0.527727 11.00000 0.01485 0.01878 = 0.01540 0.00665 0.00263 0.00156 AFIX 13 H7 2 0.060213 0.234642 0.483902 11.00000 -1.20000 AFIX 0 C10 1 0.223872 0.332851 0.638557 11.00000 0.01582 0.01895 = 0.01576 0.00752 0.00204 0.00058 C11 1 0.385576 0.319349 0.605034 11.00000 0.01578 0.02011 = 0.01719 0.00650 0.00259 -0.00070 AFIX 13 H8 2 0.460524 0.390603 0.618283 11.00000 -1.20000 AFIX 0 C12 1 0.412666 0.215187 0.646591 11.00000 0.01390 0.02220 = 0.01760 0.00788 0.00192 0.00253 AFIX 13 H9 2 0.507932 0.209716 0.690071 11.00000 -1.20000 AFIX 0 C13 1 0.343095 0.112830 0.535040 11.00000 0.01544 0.01903 = 0.01714 0.00676 0.00372 0.00362 AFIX 13 H10 2 0.386595 0.032016 0.496859 11.00000 -1.20000 AFIX 0 C14 1 0.183105 0.125460 0.568739 11.00000 0.01498 0.01730 = 0.01574 0.00527 0.00290 0.00102 AFIX 13 H11 2 0.108471 0.053809 0.554985 11.00000 -1.20000 AFIX 0 C15 1 0.253622 0.226855 0.681607 11.00000 0.01416 0.01705 = 0.01733 0.00654 0.00202 0.00188 C16 1 0.230445 0.222940 0.784517 11.00000 0.02032 0.01512 = 0.01675 0.00510 0.00217 0.00127 O2 4 0.341073 0.213893 0.842947 11.00000 0.02254 0.03548 = 0.02116 0.01473 0.00095 0.00456 N2 3 0.088730 0.226083 0.807445 11.00000 0.02032 0.02236 = 0.01677 0.00799 0.00423 0.00092 C17 1 0.061149 0.217374 0.906581 11.00000 0.02920 0.03676 = 0.02250 0.01589 0.01017 0.00367 AFIX 13 H14 2 -0.049949 0.220694 0.907349 11.00000 -1.20000 AFIX 0 C18 1 0.100041 0.092637 0.908085 11.00000 0.05519 0.05071 = 0.05185 0.03834 0.02420 0.01269 AFIX 137 H28 2 0.045828 0.024216 0.844403 11.00000 -1.50000 H29 2 0.070367 0.087023 0.970935 11.00000 -1.50000 H30 2 0.208990 0.086292 0.909886 11.00000 -1.50000 AFIX 0 C19 1 0.137468 0.330312 1.003604 11.00000 0.04214 0.05575 = 0.01749 0.01176 0.00784 0.00201 AFIX 137 H31 2 0.247240 0.327372 1.009492 11.00000 -1.50000 H32 2 0.104415 0.329040 1.067055 11.00000 -1.50000 H33 2 0.109883 0.407235 0.996730 11.00000 -1.50000 AFIX 0 C20 1 -0.043461 0.237658 0.738066 11.00000 0.01701 0.02641 = 0.01923 0.00788 0.00446 0.00144 AFIX 13 H15 2 -0.005906 0.243863 0.676174 11.00000 -1.20000 AFIX 0 C21 1 -0.154953 0.121713 0.694951 11.00000 0.02465 0.03393 = 0.02911 0.00628 0.00545 -0.00511 AFIX 137 H34 2 -0.101968 0.046936 0.661787 11.00000 -1.50000 H35 2 -0.234608 0.127537 0.642325 11.00000 -1.50000 H36 2 -0.199970 0.116116 0.753020 11.00000 -1.50000 AFIX 0 C22 1 -0.120564 0.356314 0.792505 11.00000 0.02624 0.03193 = 0.03228 0.01255 0.01081 0.00750 AFIX 137 H37 2 -0.163660 0.351477 0.851536 11.00000 -1.50000 H38 2 -0.201201 0.364551 0.741675 11.00000 -1.50000 H39 2 -0.046384 0.429170 0.819289 11.00000 -1.50000 AFIX 0 C23 1 0.162001 0.456259 0.687477 11.00000 0.01559 0.01912 = 0.01911 0.00930 0.00481 0.00025 N3 3 0.048969 0.477432 0.627327 11.00000 0.01967 0.02165 = 0.02235 0.00986 0.00285 0.00257 C24 1 -0.003913 0.593096 0.664284 11.00000 0.02052 0.02406 = 0.02756 0.01244 0.00269 0.00525 AFIX 43 H1 2 -0.085305 0.608234 0.621277 11.00000 -1.20000 AFIX 0 C25 1 0.052792 0.688116 0.758986 11.00000 0.02300 0.01938 = 0.02928 0.01066 0.00801 0.00525 AFIX 43 H2 2 0.013117 0.767481 0.779853 11.00000 -1.20000 AFIX 0 C26 1 0.171349 0.667472 0.825976 11.00000 0.01952 0.02080 = 0.02167 0.00833 0.00722 0.00005 C27 1 0.235691 0.760759 0.926768 11.00000 0.02731 0.01908 = 0.02458 0.00406 0.00801 0.00152 AFIX 43 H3 2 0.200218 0.841799 0.951080 11.00000 -1.20000 AFIX 0 C28 1 0.348047 0.734600 0.988771 11.00000 0.02928 0.02446 = 0.01936 0.00298 0.00253 -0.00390 AFIX 43 H4 2 0.389650 0.797435 1.056230 11.00000 -1.20000 AFIX 0 C29 1 0.402971 0.615313 0.953729 11.00000 0.02528 0.02660 = 0.02146 0.01001 -0.00085 -0.00223 AFIX 43 H5 2 0.480545 0.598120 0.998035 11.00000 -1.20000 AFIX 0 C30 1 0.345432 0.523890 0.856277 11.00000 0.02171 0.02002 = 0.02229 0.00873 0.00334 0.00064 AFIX 43 H6 2 0.384406 0.444174 0.832992 11.00000 -1.20000 AFIX 0 C31 1 0.228048 0.547593 0.789987 11.00000 0.01727 0.01985 = 0.01885 0.00824 0.00506 -0.00046 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM qq REM R1 = 0.0365 for 4210 Fo > 4sig(Fo) and 0.0402 for all 4665 data REM 333 parameters refined using 0 restraints END WGHT 0.0405 0.6108 REM Highest difference peak 0.267, deepest hole -0.189, 1-sigma level 0.036 Q1 1 0.3358 0.2183 0.6777 11.00000 0.05 0.27 Q2 1 0.2296 0.2218 0.4959 11.00000 0.05 0.26 Q3 1 0.3051 0.3428 0.6246 11.00000 0.05 0.25 Q4 1 0.2269 0.2859 0.6722 11.00000 0.05 0.25 Q5 1 0.3381 0.1570 0.5000 11.00000 0.05 0.24 Q6 1 0.2038 0.1710 0.6378 11.00000 0.05 0.24 Q7 1 0.3631 0.2733 0.5382 11.00000 0.05 0.24 Q8 1 0.1719 0.2916 0.5847 11.00000 0.05 0.22 Q9 1 0.2596 0.0943 0.5492 11.00000 0.05 0.22 Q10 1 0.3941 0.1547 0.5930 11.00000 0.05 0.19 Q11 1 0.1518 0.1752 0.5481 11.00000 0.05 0.19 Q12 1 0.2370 0.2327 0.7328 11.00000 0.05 0.18 Q13 1 0.3245 0.2111 0.4449 11.00000 0.05 0.18 Q14 1 0.4688 0.2146 0.3097 11.00000 0.05 0.17 Q15 1 0.2237 0.6168 0.7981 11.00000 0.05 0.17 Q16 1 0.0745 0.2230 0.8553 11.00000 0.05 0.17 Q17 1 0.4213 0.2774 0.6365 11.00000 0.05 0.17 Q18 1 -0.1003 0.1810 0.7159 11.00000 0.05 0.16 Q19 1 0.6415 0.2998 0.4508 11.00000 0.05 0.16 Q20 1 0.5361 0.2251 0.3898 11.00000 0.05 0.14 Q21 1 0.1949 0.3887 0.6616 11.00000 0.05 0.14 Q22 1 0.6595 0.1886 0.4042 11.00000 0.05 0.14 Q23 1 -0.0793 0.2946 0.7649 11.00000 0.05 0.13 Q24 1 0.0310 0.2378 0.7774 11.00000 0.05 0.13 Q25 1 0.2144 0.5083 0.7317 11.00000 0.05 0.13 ; _shelx_res_checksum 75276 _shelx_hkl_file ; 0 0 -2 13359.1 375.353 0 0 2 13036.5 374.057 0 0 2 13243.6 374.261 0 0 2 12964.9 375.183 0 0 3 873.530 26.9739 0 0 -3 863.738 28.6127 0 0 3 860.738 26.5669 0 0 3 889.415 28.4262 0 0 4 645.558 23.3769 0 0 4 703.069 21.2247 0 0 4 632.140 21.6796 0 0 4 623.159 22.6017 0 0 -4 668.568 23.9581 0 0 -5 5426.02 161.627 0 0 5 5511.34 159.050 0 0 5 5613.75 158.297 0 0 5 5245.61 160.247 0 0 6 15658.4 459.492 0 0 -6 16146.5 461.027 0 0 6 16042.7 457.849 0 0 -6 16095.7 461.101 0 0 -6 15527.2 459.223 0 0 6 16249.8 456.703 0 0 -7 8519.75 245.687 0 0 -7 8506.49 243.905 0 0 -7 8143.84 245.575 0 0 7 8075.64 244.132 0 0 7 8404.42 240.377 0 0 7 8387.46 241.899 0 0 -8 24.0157 7.61149 0 0 8 35.5020 6.42899 0 0 8 34.6703 6.99862 0 0 -8 48.3248 9.57848 0 0 8 40.0288 4.74144 0 0 -8 29.6193 7.37346 0 0 -9 372.181 20.5314 0 0 9 353.882 14.1561 0 0 -9 371.237 20.3198 0 0 9 365.645 16.1397 0 0 9 355.589 18.8202 0 0 10 42.2792 5.62393 0 0 10 54.2418 7.92445 0 0 -10 56.5520 11.4572 0 0 10 41.2094 8.90649 0 0 11 320.208 20.3080 0 0 11 322.293 13.6779 0 0 -11 332.862 21.4621 0 0 12 426.408 24.5768 0 0 12 436.952 17.0531 0 0 -12 405.953 25.3643 0 0 13 2985.49 99.9668 0 0 -13 2950.33 100.509 0 0 14 13.6007 12.2130 0 0 -14 16.8580 14.3300 0 0 -15 74.5327 17.9706 0 0 15 71.5595 17.1005 0 0 16 263.598 24.9122 0 0 -16 234.817 24.3216 0 0 -17 302.777 27.7668 0 0 17 285.105 27.7006 0 0 -18 153.862 25.8916 0 1 -18 308.921 29.6485 0 1 -17 380.053 30.4710 0 -1 17 345.991 27.6017 0 1 -16 198.220 23.7198 0 -1 16 225.920 22.6887 0 -1 15 1055.55 46.5042 0 1 -15 1029.67 47.1127 0 -1 14 17.8209 12.2881 0 1 -14 32.4350 14.8767 0 1 -13 165.911 18.5954 0 -1 13 169.710 16.8251 0 -1 12 95.9418 13.2308 0 -1 12 83.5897 7.08252 0 1 -12 97.6165 14.6921 0 -1 11 173.605 9.18603 0 -1 11 160.727 14.5200 0 -1 11 155.367 10.6342 0 1 -11 162.948 16.0438 0 -1 10 591.096 22.1977 0 -1 10 579.325 20.5894 0 1 -10 536.055 27.0518 0 -1 10 568.028 25.7595 0 -1 9 1507.89 53.3799 0 1 -9 1468.78 51.1396 0 -1 9 1532.82 47.4055 0 -1 9 1471.38 51.8920 0 -1 9 1627.35 48.8396 0 1 -9 1448.70 53.2798 0 -1 8 78.6930 7.19439 0 -1 8 93.7904 8.71791 0 -1 8 80.1213 9.43779 0 -1 8 84.2413 6.32488 0 1 -8 73.8394 8.88906 0 1 -8 70.9892 10.3329 0 1 -7 224.617 13.8984 0 -1 7 221.731 13.5143 0 -1 7 219.502 11.9858 0 1 -7 205.985 12.0719 0 -1 6 564.402 22.1452 0 1 -6 505.176 20.1113 0 -1 6 550.077 20.6083 0 1 -6 516.600 18.3970 0 -1 6 528.928 18.7250 0 1 -6 505.089 21.7953 0 1 -5 767.356 25.1756 0 1 -5 714.229 23.5147 0 -1 5 700.930 23.6091 0 -1 5 730.573 24.9899 0 1 -5 703.502 26.4757 0 -1 5 747.689 26.6829 0 -1 4 7.67097 3.41186 0 1 -4 11.0373 4.40163 0 1 -4 4.28427 3.37202 0 -1 4 2.90942 3.40404 0 1 -4 8.65522 5.78117 0 -1 4 9.14388 4.87827 0 -1 3 1577.06 48.5533 0 -1 3 1572.76 46.7225 0 -1 3 1611.32 47.4706 0 1 -3 1615.01 48.6167 0 1 -3 1525.02 46.7415 0 1 -3 1639.79 47.4780 0 1 -2 310.269 10.3983 0 -1 2 312.018 10.3581 0 1 -2 306.277 10.1135 0 1 -2 279.212 11.1288 0 -1 2 315.452 10.1190 0 1 1 295.061 10.9734 0 -1 -1 325.041 11.0758 0 -1 -1 330.524 10.4583 0 -1 -1 339.464 10.8683 0 1 1 293.648 10.4348 0 -1 -2 5814.50 165.875 0 1 2 5828.31 165.758 0 -1 -2 5918.25 164.605 0 -1 -2 5569.38 165.321 0 1 2 5581.19 164.488 0 -1 -3 1904.24 62.0695 0 -1 -3 2154.70 61.1642 0 -1 -3 2104.49 62.9184 0 1 3 2038.14 60.7649 0 1 3 2128.06 62.9417 0 -1 -4 4179.62 118.623 0 1 4 3989.62 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12 5 9.96995 17.8711 -1 -12 -5 20.5921 20.3415 1 12 6 2016.28 78.7336 -1 -13 16 42.0384 21.2219 -1 -13 15-13.4198 20.2251 1 13 -15-11.6604 17.6951 -1 -13 14 130.114 23.8659 1 13 -14 98.2318 19.3874 1 13 -13 471.554 31.5173 -1 -13 13 546.394 37.5191 -1 -13 12 2281.59 86.8915 1 13 -12 2164.30 80.9016 1 13 -11 10.6096 15.0130 -1 -13 11-8.48493 17.0142 1 13 -10 108.651 18.3196 1 13 -9 56.5162 15.5105 1 13 -8 69.8083 15.8479 1 13 -7 2.57077 12.7890 -1 -13 7 4.57590 14.0774 -1 -13 6 18.1233 15.3218 1 13 -6 15.5274 14.0739 -1 -13 5 32.5320 16.5346 -1 -13 4 4.72272 15.9040 1 13 -3 596.600 33.2235 -1 -13 3 668.983 38.0062 1 13 -2 158.785 19.9157 -1 -13 2 246.443 24.0056 1 13 -1 17.3174 14.2035 -1 -13 1 14.4525 16.8278 1 13 0 244.896 22.9680 -1 -13 0 280.121 26.8822 1 13 1 566.827 33.1557 -1 -13 -1 565.877 36.9883 -1 -13 -2 41.1332 19.4692 1 13 2 9.62518 16.3058 -1 -13 -3 411.730 32.5975 1 13 3 385.944 28.7533 1 13 4 690.061 38.4361 1 14 -15 29.2139 18.4370 -1 -14 14 585.525 40.0581 1 14 -14 518.904 34.5006 -1 -14 13 1267.38 61.8316 1 14 -13 1341.00 57.2931 1 14 -12 1225.14 54.7474 -1 -14 12 1291.07 60.8441 1 14 -11 367.311 27.8802 1 14 -10 117.836 19.8292 1 14 -9 366.756 27.5172 -1 -14 8 44.3901 20.1414 1 14 -8 25.1491 15.2153 -1 -14 7 650.722 39.2293 1 14 -7 658.448 36.5802 1 14 -6 714.043 37.7268 -1 -14 6 643.969 39.1805 -1 -14 5 318.096 28.7577 -1 -14 4 10.4635 18.0134 1 14 -4 11.5674 13.8785 -1 -14 3-10.4967 17.6768 1 14 -3-13.1330 15.9691 -1 -14 2 831.976 44.4264 1 14 -2 736.045 39.8086 1 14 -1-4.44774 16.2751 -1 -14 1 31.1284 19.3427 -1 -14 0 326.913 31.1685 1 14 0 360.663 27.8011 1 14 1 7.47874 16.6252 -1 -14 -1-10.9516 19.5171 1 15 -15-11.3884 20.1572 1 15 -14 408.883 31.9446 1 15 -13 60.4941 19.8451 1 15 -12 214.521 24.9071 -1 -15 12 253.026 29.5831 1 15 -11 250.328 26.1067 1 15 -10 12.3915 17.2733 1 15 -9 54.0032 19.1357 -1 -15 9 62.5707 22.4045 -1 -15 8 585.661 39.0520 1 15 -8 599.216 36.0961 1 15 -7 2673.52 95.7318 -1 -15 7 2537.33 98.2695 -1 -15 6 285.492 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806.678 35.5796 2 -12 8 902.033 43.5088 2 -12 9 749.394 40.8773 -2 12 -9 758.147 33.9704 -2 12 -10 1767.75 64.3969 2 -12 10 1899.98 73.7140 -2 12 -11 1614.07 59.9901 2 -12 11 1685.22 69.5743 -2 12 -12 1975.78 70.3178 2 -12 12 2013.74 80.5913 2 -12 13 63.0779 21.5731 2 -12 14 31.2696 21.4693 -2 11 8 1388.88 56.5319 -2 11 7 176.967 19.8416 -2 11 6-4.50169 13.5174 2 -11 -6 2.50491 15.1230 2 -11 -5-1.24450 14.8279 -2 11 5 4.37273 12.8478 2 -11 -4 1739.63 67.0994 -2 11 4 1819.26 64.1921 -2 11 4 1797.89 65.4941 -2 11 3 324.237 20.2094 -2 11 3 301.726 21.8475 2 -11 -3 330.880 24.1467 -2 11 2 495.305 24.3650 2 -11 -2 500.543 28.9308 -2 11 2 490.058 27.0185 2 -11 -1 197.448 18.9335 -2 11 1 178.910 16.6546 -2 11 1 186.446 14.2163 2 -11 0 471.498 27.6284 -2 11 0 425.340 24.0265 2 -11 1 1603.65 61.0068 2 -11 2 6.85796 12.2221 -2 11 -2 1.82921 10.2292 -2 11 -3 1144.40 43.4572 2 -11 3 1012.42 45.5298 -2 11 -4 54.9818 11.4581 2 -11 4 64.1696 14.3674 2 -11 5 113.948 17.2918 -2 11 -5 132.249 14.0067 2 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240.424 22.2761 2 -9 10 265.807 11.9989 2 -9 11 1749.73 70.8946 -2 9 -11 1909.96 62.6413 -2 9 -12 316.666 18.5117 2 -9 15 493.458 34.1928 2 -9 16 47.7444 19.0812 2 -9 17 950.980 52.0475 -2 8 11 2.86184 16.4869 -2 8 10 264.187 24.4469 -2 8 10 281.627 21.0012 -2 8 9 30.4864 11.7945 -2 8 9 31.6634 15.1036 2 -8 -9 9.00787 13.6146 -2 8 8 83.0760 15.3855 -2 8 8 104.181 13.8484 2 -8 -8 73.7179 14.7222 -2 8 7 152.513 16.2470 2 -8 -7 171.382 17.0744 -2 8 7 157.429 15.0164 2 -8 -6 531.580 27.3713 -2 8 6 542.817 26.7488 -2 8 6 599.041 28.3297 -2 8 5 1061.55 39.8915 -2 8 5 1002.33 39.4265 2 -8 -4 36.5456 10.3937 -2 8 4 57.1482 10.6450 -2 8 4 57.3559 10.8429 -2 8 3 75.8699 10.5731 -2 8 3 75.4021 10.0933 2 -8 -3 87.2255 11.8551 2 -8 -3 81.2213 10.0214 -2 8 2 2245.57 70.4392 -2 8 2 2248.17 73.3443 2 -8 -2 2178.54 69.6403 2 -8 -2 2204.52 74.2250 2 -8 -1 2389.39 80.3938 2 -8 -1 2460.32 75.1971 -2 8 1 2439.60 78.8701 -2 8 1 2508.99 79.6805 -2 8 1 2437.76 75.6736 2 -8 0 39.5243 9.67720 -2 8 0 36.3073 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1397.55 49.8446 -2 7 2 1481.21 48.0086 2 -7 -2 1413.11 50.2041 -2 7 1 285.195 13.4084 -2 7 1 284.380 15.8694 2 -7 -1 308.984 16.8925 2 -7 -1 273.490 12.9495 -2 7 1 284.788 15.9885 2 -7 0 2740.86 88.9471 -2 7 0 2757.06 84.1996 -2 7 0 2886.69 87.8621 2 -7 0 2905.93 84.0735 -2 7 -1 1436.23 43.0718 -2 7 -1 1377.36 47.0640 -2 7 -1 1303.30 46.8021 2 -7 1 1415.10 47.4550 2 -7 1 1419.33 49.0082 2 -7 1 1400.26 42.6266 -2 7 -2 577.965 19.0074 -2 7 -2 609.491 24.3244 2 -7 2 658.579 24.5547 -2 7 -2 657.239 24.2030 2 -7 2 587.043 25.0895 2 -7 2 581.069 18.6408 -2 7 -3 731.491 28.4810 -2 7 -3 742.737 27.5071 2 -7 3 754.058 27.8817 2 -7 3 713.772 29.7903 -2 7 -4 24.2271 6.03678 2 -7 4 28.9820 8.11165 2 -7 4 28.1882 6.96048 -2 7 -4 41.2485 8.41537 -2 7 -5 1833.04 60.6160 2 -7 5 1892.85 58.3485 -2 7 -5 1735.18 57.7695 2 -7 5 1913.14 63.3826 -2 7 -6 5688.50 142.873 -2 7 -6 5562.85 138.743 2 -7 6 5724.35 146.616 2 -7 6 5778.34 139.126 -2 7 -7 262.146 13.5832 -2 7 -7 278.596 10.6943 2 -7 7 288.126 14.1564 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579.935 36.8683 -10 0 4 637.302 33.1368 10 0 -3 258.161 25.6531 -10 0 3 302.021 22.4898 -10 0 2 7.01863 13.1254 10 0 -2 14.4203 16.4304 -10 0 1 103.839 16.3533 10 0 -1 79.9050 19.2261 -10 0 0 673.746 34.6782 10 0 0 698.664 37.8907 -10 0 -1 380.642 26.5240 10 0 1 465.191 30.1148 -10 0 -2 510.943 30.7466 -10 0 -2 478.835 25.9004 10 0 2 476.391 29.7760 -10 0 -3 78.8557 16.7878 -10 0 -3 67.6091 14.6432 -10 0 -4-8.51295 16.9050 -10 0 -4 1.11372 13.7281 -10 0 -5 345.169 27.2514 -10 0 -5 270.397 23.1967 -10 0 -6 2.88404 16.2260 -10 0 -6 1.32916 15.3143 -10 0 -7 277.160 25.8443 10 0 8 1629.67 72.0001 -10 0 -8 1900.10 72.4036 -10 -1 12 450.715 35.7221 -10 -1 12 394.732 29.5324 -10 -1 11 99.1661 18.1456 10 1 -11 89.6953 23.7123 -10 -1 10 105.097 18.6121 10 1 -9 337.148 31.8588 -10 -1 9 339.037 26.0441 -10 -1 8 112.121 18.6576 10 1 -8 95.8332 21.5134 10 1 -7 482.670 34.9240 -10 -1 7 447.245 28.4200 10 1 -6 5591.39 179.601 -10 -1 6 5347.95 171.946 -10 -1 5 339.554 24.7616 10 1 -5 371.665 30.2020 10 1 -4-3.37515 16.0594 -10 -1 4 12.2123 13.4482 10 1 -3 81.2683 19.0237 -10 -1 3 52.0377 14.1354 -10 -1 2 534.581 30.9111 10 1 -2 488.560 33.1569 -10 -1 1 1167.13 49.7412 10 1 -1 1093.13 50.9795 10 1 0-4.28581 16.8831 -10 -1 0 10.6760 15.8144 10 1 1 164.156 20.6269 -10 -1 -1 161.366 20.6744 -10 -1 -1 164.842 16.2099 -10 -1 -2 34.5769 16.3762 -10 -1 -2 64.9298 14.3481 -10 -1 -3 114.071 20.3661 -10 -1 -3 156.680 17.6452 -10 -1 -4 12.0997 17.5045 -10 -1 -4 52.7639 15.9962 -10 -1 -5 218.671 23.9656 -10 -1 -5 207.189 22.5409 -10 -1 -6 33.7331 17.4820 10 1 7 160.362 24.6129 -10 -1 -7 213.329 24.7890 -10 -2 12 603.515 36.2960 10 2 -11 646.924 42.3253 -10 -2 11 602.755 36.0755 -10 -2 10 622.569 35.3827 -10 -2 9 1188.19 51.2781 10 2 -9 1078.61 55.5444 -10 -2 8 26.9888 14.8654 10 2 -8-1.89004 17.5274 -10 -2 7 123.027 18.1750 10 2 -7 121.494 22.0300 -10 -2 6 405.049 28.5212 10 2 -6 492.786 34.7190 -10 -2 5 394.461 26.7064 10 2 -5 434.896 32.1844 -10 -2 4 704.590 36.7193 10 2 -4 790.126 42.3808 10 2 -3 16.3984 18.3959 -10 -2 3-14.6228 15.1831 10 2 -2-14.1536 16.0674 -10 -2 2-5.41279 15.5482 -10 -2 1 2112.04 78.8863 10 2 -1 2116.49 79.8820 10 2 0 266.958 25.0240 -10 -2 0 271.663 19.8522 -10 -2 -1 463.657 30.4319 10 2 1 433.219 29.2400 -10 -2 -1 413.101 25.4221 -10 -2 -2 126.078 19.9751 -10 -2 -2 124.527 16.9499 -10 -2 -3 745.143 40.2928 -10 -2 -3 643.643 34.1537 -10 -2 -4 11.1504 18.8938 -10 -2 -4 43.2947 17.2277 -10 -2 -5 31.8138 18.2445 -10 -2 -5 33.0243 15.9720 10 2 6 34.2801 19.8807 -10 -2 -6 22.2140 16.5291 -10 -2 -7 96.6940 21.7301 10 3 -12 730.563 47.0706 -10 -3 12 894.142 44.5791 -10 -3 11 361.299 28.9073 10 3 -11 313.950 31.3977 -10 -3 10-12.0216 16.6018 -10 -3 9 122.596 19.2132 10 3 -9 122.050 23.0938 10 3 -8 44.1247 19.9132 -10 -3 8 33.7887 15.8777 10 3 -7 35.7215 17.9075 -10 -3 7 22.5992 15.6704 10 3 -6 2986.11 110.145 -10 -3 6 3062.01 105.278 10 3 -5 156.982 22.7780 -10 -3 5 146.836 19.0088 10 3 -4 10.3754 17.4109 -10 -3 4 22.4136 14.0543 10 3 -3 718.893 41.3038 -10 -3 3 783.442 39.5434 10 3 -2 91.3228 19.0764 -10 -3 2 46.3715 17.3189 10 3 -1 78.0798 18.8872 -10 -3 1 92.2077 19.6083 10 3 0 802.649 41.9190 -10 -3 0 885.278 43.6515 -10 -3 0 803.418 36.9052 10 3 1 472.116 31.8121 -10 -3 -1 497.231 33.7570 -10 -3 -1 537.048 29.0173 -10 -3 -2 48.4057 19.3339 -10 -3 -2 55.4312 15.9074 -10 -3 -3-8.23923 18.1443 -10 -3 -3 7.69360 15.6852 -10 -3 -4 298.242 28.0518 -10 -3 -4 310.493 25.9247 -10 -3 -5 255.273 25.9855 -10 -3 -5 238.023 24.3705 -10 -3 -6 708.807 39.8783 -10 -4 12-4.81284 16.3890 10 4 -12 16.5024 20.2835 -10 -4 11 20.5618 17.0918 -10 -4 10 24.3829 17.1095 10 4 -9 109.772 22.8055 -10 -4 9 78.0186 19.2624 10 4 -8 131.366 23.7132 -10 -4 8 129.415 20.1460 10 4 -7 113.446 22.9280 -10 -4 7 103.889 19.6680 10 4 -6 481.144 35.7603 -10 -4 6 486.896 31.2561 10 4 -5 180.832 24.8290 -10 -4 5 188.137 21.6472 -10 -4 4-7.44048 15.2022 10 4 -4 1.76977 17.6763 -10 -4 3 244.997 24.1715 10 4 -3 248.993 26.2160 -10 -4 2 315.158 27.5392 10 4 -2 339.264 28.2007 -10 -4 1 4757.69 153.616 10 4 -1 4491.17 152.297 -10 -4 1 4595.93 145.509 -10 -4 0 2119.66 81.3989 -10 -4 0 2099.13 74.7147 10 4 0 2039.71 78.9558 -10 -4 -1 94.7122 19.6702 -10 -4 -1 142.895 19.0623 -10 -4 -2 33.9002 19.0283 -10 -4 -2 76.1505 16.6842 -10 -4 -3 89.4529 21.9062 -10 -4 -3 146.922 20.2418 -10 -4 -4 29.4824 18.2444 -10 -4 -4 21.9863 16.5087 -10 -4 -5 11.0061 18.6853 10 5 -12 44.4905 22.1424 -10 -5 12 34.8276 19.6299 -10 -5 11 714.276 40.0978 10 5 -10 16.5541 20.3470 -10 -5 10-6.35998 16.4211 10 5 -9 126.541 23.2914 -10 -5 9 143.877 21.4944 -10 -5 8 261.523 25.8083 10 5 -8 186.855 25.4810 -10 -5 7 100.026 19.5978 10 5 -7 206.293 25.5981 -10 -5 6 275.337 25.2566 10 5 -6 288.838 28.9138 10 5 -5 3.76938 20.2205 -10 -5 5 6.23968 16.5117 10 5 -4 36.5635 18.6925 -10 -5 4 78.9591 17.9122 -10 -5 3 569.992 35.1868 10 5 -3 577.538 37.0814 -10 -5 2 1211.78 55.4425 10 5 -2 1270.68 57.0901 -10 -5 2 1202.63 49.5797 -10 -5 1 12.7259 15.2450 10 5 -1 9.74588 17.7231 -10 -5 1 35.5238 19.0422 -10 -5 0 1529.95 67.3897 10 5 0 1579.55 65.6779 -10 -5 0 1638.26 62.1983 -10 -5 -1 43.3303 20.0772 -10 -5 -1 55.5035 16.7545 -10 -5 -2-10.6209 17.4082 -10 -5 -2 28.9832 16.7550 -10 -5 -3 540.092 36.9656 -10 -5 -3 507.956 33.2325 -10 -5 -4 6.19450 18.6998 10 6 -10 148.362 24.9187 10 6 -9 227.341 27.6123 10 6 -8 316.942 30.5566 10 6 -7 14.2804 19.3356 -10 -6 7 17.8908 17.5715 10 6 -6 72.1238 20.0514 -10 -6 6 29.3583 17.3705 10 6 -5 23.4790 20.3356 -10 -6 5 70.7088 19.4381 -10 -6 4 74.8134 18.5283 10 6 -4 146.224 24.8947 -10 -6 3 241.655 25.7842 10 6 -3 183.167 25.6125 -10 -6 2 612.862 38.1335 10 6 -2 662.553 40.2872 -10 -6 2 616.629 33.5433 -10 -6 1 166.377 21.0028 -10 -6 1 145.503 23.3701 10 6 -1 165.755 23.4377 -10 -6 0 1.34748 15.9240 -10 -6 -1 35.2202 17.7441 -10 -6 -1 39.7736 19.6814 -10 -6 -2 283.381 25.2723 -10 -6 -3-7.87537 19.4159 10 7 -10 72.2140 24.0586 -10 -7 10 32.9767 19.6961 10 7 -9 52.0166 23.3766 10 7 -8 4.28595 20.3054 10 7 -7 61.2539 22.5762 10 7 -6 94.6765 23.1745 10 7 -5 307.418 32.1466 10 7 -4 62.6358 22.6871 10 7 -3-7.54975 19.9788 10 7 -2 905.053 47.3186 -10 -7 2 857.629 41.4219 -10 -7 1 112.158 19.4108 -10 -7 1 69.0820 21.5062 10 7 -1 71.7725 21.6626 -10 -7 0 10.1837 17.6607 -10 -7 -1 13.7751 19.0124 -10 -8 9 205.492 25.9360 10 8 -9 191.709 27.5055 -10 -8 8 8.88434 17.8838 10 8 -8 2.20139 21.7325 -10 -8 7 147.252 22.6700 10 8 -7 164.225 27.1224 -10 -8 6 1340.89 61.3884 10 8 -6 1327.00 64.5479 -10 -8 5 148.709 24.4833 10 8 -5 159.808 26.1408 10 8 -4 225.735 28.5200 -10 -8 4 169.750 24.4872 10 8 -3 702.624 44.2512 -10 -8 3 681.981 38.3127 10 8 -2 503.702 38.1931 -10 -8 2 522.637 34.2512 -10 -8 1 9.04724 16.8139 -10 -8 0 181.114 24.5192 10 9 -6 165.969 28.5065 10 9 -5 1700.69 76.3974 10 9 -4 230.891 29.9709 -10 -9 3 29.2870 18.7809 10 9 -3 36.9357 23.3164 -10 -9 2 23.9111 19.5089 10 9 -2 17.9147 21.9259 -11 9 -2 12.4639 14.9256 -11 8 0 1003.34 44.5762 -11 8 -1 481.846 28.7773 -11 8 -2 6.49641 13.6471 -11 7 2 141.410 19.2005 -11 7 1 2976.59 101.890 -11 7 0 3283.52 109.819 -11 7 -1 407.417 25.8752 -11 7 -2 562.960 29.8458 -11 6 3 16.2307 15.5004 -11 6 2 547.781 32.2012 -11 6 1 242.289 22.2053 -11 6 0 787.177 38.2368 -11 6 -1 41.0880 14.4428 -11 6 -2 23.2994 13.2085 -11 5 5 40.4008 16.4712 -11 5 4 102.037 18.7802 -11 5 3 46.1169 16.2119 -11 5 2 13.8149 14.5172 -11 5 1 1728.80 65.3999 -11 5 0 1533.46 59.1837 -11 5 -1 8.50902 13.3424 -11 5 -2 113.837 15.7729 -11 4 6 98.5209 19.3325 -11 4 5 5.98266 15.3361 -11 4 4 738.504 39.6195 -11 4 3 108.450 18.9966 -11 4 2 68.5621 16.7677 -11 4 1 1407.27 56.3549 -11 4 0 3.45043 13.3284 -11 4 -1 79.7446 15.4463 -11 3 9 13.8968 15.2594 -11 3 8 294.512 25.0224 -11 3 7 148.055 23.1012 -11 3 7 105.078 17.9253 -11 3 6 489.570 33.1528 -11 3 6 448.315 28.5751 -11 3 5 113.251 20.2857 -11 3 5 51.0464 15.8767 -11 3 4 874.858 44.0498 -11 3 3 534.914 33.4147 -11 3 3 572.825 30.5906 -11 3 2 29.7801 15.7483 -11 3 2 22.7507 14.2227 -11 3 1 343.678 25.1396 -11 3 0 19.9795 13.6309 -11 3 -1 55.5049 14.8088 -11 2 10 52.7950 18.4699 -11 2 9 41.3528 16.6493 -11 2 8 480.780 34.9227 -11 2 8 469.398 29.8154 -11 2 7 287.581 28.0125 -11 2 7 273.451 23.9915 -11 2 6 272.890 27.5176 -11 2 6 249.403 22.6185 -11 2 5 3402.72 117.478 -11 2 5 3330.26 112.486 -11 2 4 127.702 20.3721 -11 2 4 143.314 18.7181 -11 2 3 2052.39 76.9123 -11 2 3 1934.83 71.7344 -11 2 2 1191.30 50.4748 -11 2 2 1073.46 47.2810 -11 2 1 354.258 25.9135 -11 2 1 358.960 24.8678 -11 2 0 131.688 17.8707 -11 2 0 149.606 17.6071 -11 2 -1 128.461 18.4707 -11 2 -1 157.153 18.2116 -11 2 -2 192.510 20.0907 -11 1 10 11.2208 16.6693 -11 1 9 138.976 20.6800 -11 1 8 271.179 27.9823 -11 1 8 285.249 24.9341 -11 1 7 24.1047 18.4852 -11 1 7 24.9622 16.3717 -11 1 6 1105.21 51.7103 -11 1 6 983.837 46.5573 -11 1 5 4337.54 140.028 -11 1 5 3950.75 133.958 -11 1 4 64.9767 19.1965 -11 1 4 44.1144 15.8491 -11 1 3 1262.48 55.0747 -11 1 3 1291.31 53.3643 -11 1 2 9.54978 15.4899 -11 1 2-3.65916 14.8050 -11 1 1 298.976 24.3072 -11 1 1 354.671 25.2383 -11 1 0 116.620 17.2068 -11 1 0 91.4074 17.4113 -11 1 -1 607.052 31.8240 -11 1 -1 660.379 35.5060 -11 1 -2 149.057 20.2383 -11 1 -3 4.19737 16.1208 -11 1 -4 402.847 30.2944 -11 1 -5 299.765 26.4096 -11 0 10 42.8795 17.1648 -11 0 9 316.363 29.9670 -11 0 8 4723.45 152.670 -11 0 8 4279.27 145.484 -11 0 7 5156.92 165.233 11 0 -6 73.7704 22.7447 -11 0 6 35.5106 15.3002 11 0 -5-7.77451 19.6377 -11 0 5 20.7399 14.7211 11 0 -4 252.062 28.3416 -11 0 3 722.613 36.7484 11 0 -3 713.904 42.8317 -11 0 2 275.054 23.6905 11 0 -2 259.130 27.4285 -11 0 1 2642.72 95.1048 11 0 -1 2803.82 100.313 11 0 0 1897.02 74.9620 -11 0 0 1902.23 72.4470 -11 0 -1 743.925 39.5984 -11 0 -2 123.143 20.7223 -11 0 -3 144.744 23.3001 -11 0 -4 686.279 39.3684 -11 0 -5 34.3845 18.1893 -11 0 -6 784.034 43.0402 -11 -1 10 237.912 24.1850 -11 -1 9 1467.93 61.8031 11 1 -9 1524.01 69.7670 -11 -1 8 784.680 40.4281 11 1 -8 739.183 46.4562 11 1 -7 312.886 30.5579 -11 -1 7 272.414 24.0217 -11 -1 6 19.1914 16.0340 11 1 -6 30.1390 20.3087 -11 -1 5-13.8541 16.3281 11 1 -5 7.78372 20.0976 11 1 -4 91.7387 22.0372 -11 -1 4 118.875 18.9128 11 1 -3 938.979 48.7003 -11 -1 3 920.003 43.8972 11 1 -2 57.1015 20.4230 -11 -1 2 28.2047 16.6574 11 1 -1 374.271 30.1426 -11 -1 1 351.970 27.8809 11 1 0 773.766 40.6770 -11 -1 0 626.523 37.9929 -11 -1 -1 72.9724 18.7133 -11 -1 -2 1047.83 50.9853 -11 -1 -3 347.445 29.5669 -11 -1 -4 134.070 23.6866 -11 -1 -5 626.804 39.0761 -11 -2 10 129.718 20.7108 11 2 -9 85.5261 24.4172 -11 -2 9 51.7578 19.1800 11 2 -8 2629.42 100.131 -11 -2 8 2473.48 91.3080 11 2 -7 646.298 41.6991 -11 -2 7 569.418 34.7206 11 2 -6 98.8055 23.4059 -11 -2 6 73.0132 18.7712 -11 -2 5 86.8194 18.6885 11 2 -5 105.611 23.2764 -11 -2 4 24.7033 17.4901 11 2 -4 64.7831 21.8430 -11 -2 3 155.476 21.5535 11 2 -3 181.442 24.2949 -11 -2 2 109.449 20.7715 11 2 -2 129.556 21.8463 -11 -2 1 1668.19 69.3879 11 2 -1 1796.12 71.2907 -11 -2 0 1545.54 64.8110 11 2 0 1464.22 62.6548 -11 -2 -1 4.96605 18.5136 -11 -2 -2 336.682 30.1811 -11 -3 10 22.6853 18.5725 -11 -3 9 1581.22 65.7159 11 3 -9 1606.71 72.3679 -11 -3 8 663.164 38.0064 11 3 -8 707.740 44.3517 -11 -3 7 661.309 38.3526 11 3 -7 727.230 44.1649 -11 -3 6 469.904 32.6062 11 3 -6 460.739 36.7617 11 3 -5 23.4265 21.2219 -11 -3 5-10.6082 16.8966 11 3 -4 18.8165 18.8128 -11 -3 4 37.1504 17.3329 11 3 -3 3.61324 18.4560 -11 -3 3 3.17008 17.5081 11 3 -2 1.72968 17.4089 -11 -3 2-12.9869 18.6507 -11 -3 1 300.444 27.5047 11 3 -1 329.833 28.7757 -11 -3 0 22.2726 18.6352 -11 -3 -1 654.900 40.7090 -11 -3 -2 143.140 24.6684 -11 -3 -3 149.894 25.8608 11 4 -9 30.3418 22.0723 -11 -4 9 25.9998 17.3348 11 4 -8 34.3828 20.8691 -11 -4 8 82.4742 19.9130 11 4 -7 537.561 39.4818 -11 -4 7 574.972 36.4875 11 4 -6 1009.72 53.3195 -11 -4 6 955.877 47.8092 11 4 -5 776.781 46.3179 -11 -4 5 793.093 42.7300 11 4 -4 727.243 43.4436 -11 -4 4 684.219 40.2385 11 4 -3 16.6785 19.4182 -11 -4 3 16.8370 18.8362 11 4 -2 51.3974 21.2109 -11 -4 2 39.5532 19.1558 11 4 -1 2183.76 82.2162 -11 -4 1 1981.35 81.6116 -11 -4 0 1573.98 68.2028 -11 -4 -1-1.84971 20.8134 -11 -5 9 689.053 40.3430 11 5 -8 556.501 40.8945 -11 -5 8 509.550 36.1050 -11 -5 7 27.0134 18.5471 11 5 -6 6.34049 20.9497 -11 -5 6 18.5916 17.7090 11 5 -5 36.9506 20.2802 -11 -5 5 92.2048 21.2964 -11 -5 4 111.252 22.9114 11 5 -4 81.3046 22.3544 -11 -5 3 509.364 35.3722 11 5 -3 539.889 38.5250 -11 -5 2 2981.43 108.571 11 5 -2 2933.02 108.387 -11 -5 1 12.8787 19.8075 11 6 -7 193.433 30.1688 -11 -6 6 239.592 26.8015 11 6 -6 205.684 29.7138 11 6 -5 36.1325 23.4255 11 6 -4 55.6107 23.4419 -11 -6 4 58.4554 21.0492 11 6 -3 3087.75 114.655 11 6 -2 143.870 26.4833 11 7 -6 15.7419 22.3787 11 7 -5 48.2553 22.9370 11 7 -4 68.1904 27.0554 11 7 -3 2533.52 99.8815 -12 6 0 1746.95 66.7015 -12 5 1 34.7042 16.1510 -12 5 0 312.810 24.3190 -12 4 3 4.40388 16.3168 -12 4 2 36.2279 17.0317 -12 4 1 277.345 24.5527 -12 4 0 255.191 22.6681 -12 3 4 177.576 23.0610 -12 3 3 121.545 20.5321 -12 3 2 16.8665 16.3411 -12 3 1 57.0313 17.1910 -12 3 0 162.531 20.1000 -12 2 5 936.566 48.3078 -12 2 4 44.9369 18.9045 -12 2 3 53.4513 18.7902 -12 2 2 546.272 34.0817 -12 2 1 858.498 42.3276 -12 2 0 20.3049 15.2128 -12 1 8 1275.90 56.3919 -12 1 7 1617.14 65.4998 -12 1 6 1872.96 72.9289 -12 1 5 225.976 25.5775 -12 1 5 268.754 24.6324 -12 1 4 56.4009 19.6123 -12 1 4 83.3833 19.0298 -12 1 3 652.676 37.5144 -12 1 3 603.138 34.7877 -12 1 2 220.294 23.3036 -12 1 2 178.981 22.3576 -12 1 1 8.24686 15.5620 -12 1 1 12.2426 16.6421 -12 0 8 2684.22 97.1853 -12 0 7 28.2893 19.6237 -12 0 6 2959.76 106.971 -12 0 6 2886.55 101.983 -12 0 5 73.9643 20.5070 -12 0 5 71.0514 18.8668 -12 0 4-1.61045 17.9029 -12 0 4 22.8387 18.1227 -12 0 3 36.9769 18.5535 -12 0 3 93.9597 19.5962 -12 0 2 67.5554 18.4036 -12 0 2 49.1006 18.0109 -12 0 1 83.5727 19.2881 -12 0 1 62.3117 18.9028 -12 0 0 575.461 35.3470 -12 0 -1 34.8259 18.6304 -12 0 -2 123.281 23.4373 -12 0 -3 489.642 35.4495 -12 -1 7 3859.35 130.185 -12 -1 6 76.4621 19.2549 12 1 -6 43.2641 24.1139 -12 -1 5 510.838 33.5219 12 1 -5 557.171 40.0200 12 1 -4 2.03576 20.6447 -12 -1 4 13.9525 17.7083 12 1 -3-3.91554 21.2189 -12 -1 3-25.8845 18.1483 -12 -1 2 1199.50 55.9256 12 1 -2 1311.28 60.2579 -12 -1 1 1836.33 73.9084 -12 -1 0 280.787 28.0327 -12 -1 -1 363.446 30.6355 -12 -1 -2 779.024 44.8642 -12 -2 7 456.790 33.0451 12 2 -6 158.374 28.1615 -12 -2 6 134.994 22.6280 12 2 -5 341.679 32.7335 -12 -2 5 309.775 28.6181 12 2 -4 810.372 47.7383 -12 -2 4 787.430 43.2559 12 2 -3 543.534 38.5991 -12 -2 3 510.180 35.3451 12 2 -2 24.0631 20.1244 -12 -2 2 3.38712 19.0592 -12 -2 1 352.730 31.5270 -12 -2 0 198.742 27.3430 -12 -3 5 648.099 39.3819 12 3 -5 701.344 44.5738 -12 -3 4 611.570 39.0402 12 3 -4 711.139 43.8612 -12 -3 3 597.523 38.6632 12 3 -3 553.674 38.9207 12 3 -2 469.340 35.5880 12 4 -5 582.208 42.1137 12 4 -4 363.878 34.6242 12 5 -3 243.570 30.2320 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 75175 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.21084(10) 0.17454(8) 0.31688(7) 0.0224(2) Uani 1 1 d . . . . . C1 C 0.32744(13) 0.20078(11) 0.38159(9) 0.0173(3) Uani 1 1 d . . . . . N1 N 0.46553(11) 0.21333(10) 0.35656(8) 0.0193(2) Uani 1 1 d . . . . . C2 C 0.60644(14) 0.23449(12) 0.43098(10) 0.0217(3) Uani 1 1 d . . . . . H12 H 0.579207 0.226704 0.495089 0.026 Uiso 1 1 calc R U . . . C3 C 0.71476(16) 0.13510(14) 0.38475(12) 0.0313(3) Uani 1 1 d . . . . . H16 H 0.660862 0.051744 0.357021 0.047 Uiso 1 1 calc R U . . . H17 H 0.798537 0.142536 0.440184 0.047 Uiso 1 1 calc R U . . . H18 H 0.754367 0.147270 0.327398 0.047 Uiso 1 1 calc R U . . . C4 C 0.68177(16) 0.36607(13) 0.46689(12) 0.0302(3) Uani 1 1 d . . . . . H19 H 0.705912 0.378201 0.405311 0.045 Uiso 1 1 calc R U . . . H20 H 0.774825 0.376969 0.516316 0.045 Uiso 1 1 calc R U . . . H21 H 0.612999 0.427646 0.502128 0.045 Uiso 1 1 calc R U . . . C5 C 0.47807(16) 0.20718(13) 0.25005(10) 0.0256(3) Uani 1 1 d . . . . . H13 H 0.587262 0.226927 0.250581 0.031 Uiso 1 1 calc R U . . . C6 C 0.39364(18) 0.30666(16) 0.22826(13) 0.0374(4) Uani 1 1 d . . . . . H22 H 0.284830 0.287329 0.221296 0.056 Uiso 1 1 calc R U . . . H23 H 0.416954 0.308422 0.162506 0.056 Uiso 1 1 calc R U . . . H24 H 0.424583 0.388538 0.286905 0.056 Uiso 1 1 calc R U . . . C7 C 0.43443(19) 0.07573(15) 0.16351(11) 0.0390(4) Uani 1 1 d . . . . . H25 H 0.495442 0.016136 0.180227 0.058 Uiso 1 1 calc R U . . . H26 H 0.452549 0.073978 0.095524 0.058 Uiso 1 1 calc R U . . . H27 H 0.327279 0.052664 0.159199 0.058 Uiso 1 1 calc R U . . . C8 C 0.31420(13) 0.21709(11) 0.49230(9) 0.0168(3) Uani 1 1 d . . . . . C9 C 0.15547(13) 0.22980(11) 0.52773(9) 0.0165(3) Uani 1 1 d . . . . . H7 H 0.060213 0.234642 0.483902 0.020 Uiso 1 1 calc R U . . . C10 C 0.22387(13) 0.33285(11) 0.63856(9) 0.0168(3) Uani 1 1 d . . . . . C11 C 0.38558(13) 0.31935(11) 0.60503(9) 0.0181(3) Uani 1 1 d . . . . . H8 H 0.460524 0.390603 0.618283 0.022 Uiso 1 1 calc R U . . . C12 C 0.41267(13) 0.21519(11) 0.64659(9) 0.0181(3) Uani 1 1 d . . . . . H9 H 0.507932 0.209716 0.690071 0.022 Uiso 1 1 calc R U . . . C13 C 0.34310(13) 0.11283(11) 0.53504(9) 0.0173(3) Uani 1 1 d . . . . . H10 H 0.386595 0.032016 0.496859 0.021 Uiso 1 1 calc R U . . . C14 C 0.18311(13) 0.12546(11) 0.56874(9) 0.0165(3) Uani 1 1 d . . . . . H11 H 0.108471 0.053809 0.554985 0.020 Uiso 1 1 calc R U . . . C15 C 0.25362(13) 0.22686(11) 0.68161(9) 0.0164(3) Uani 1 1 d . . . . . C16 C 0.23044(14) 0.22294(11) 0.78452(9) 0.0180(3) Uani 1 1 d . . . . . O2 O 0.34107(10) 0.21389(9) 0.84295(7) 0.0256(2) Uani 1 1 d . . . . . N2 N 0.08873(12) 0.22608(10) 0.80744(8) 0.0197(2) Uani 1 1 d . . . . . C17 C 0.06115(16) 0.21737(14) 0.90658(11) 0.0277(3) Uani 1 1 d . . . . . H14 H -0.049949 0.220694 0.907349 0.033 Uiso 1 1 calc R U . . . C18 C 0.1000(2) 0.09264(17) 0.90809(14) 0.0452(4) Uani 1 1 d . . . . . H28 H 0.045828 0.024216 0.844403 0.068 Uiso 1 1 calc R U . . . H29 H 0.070367 0.087023 0.970935 0.068 Uiso 1 1 calc R U . . . H30 H 0.208990 0.086292 0.909886 0.068 Uiso 1 1 calc R U . . . C19 C 0.13747(19) 0.33031(17) 1.00360(11) 0.0393(4) Uani 1 1 d . . . . . H31 H 0.247240 0.327372 1.009492 0.059 Uiso 1 1 calc R U . . . H32 H 0.104415 0.329040 1.067055 0.059 Uiso 1 1 calc R U . . . H33 H 0.109883 0.407235 0.996730 0.059 Uiso 1 1 calc R U . . . C20 C -0.04346(14) 0.23766(12) 0.73807(10) 0.0212(3) Uani 1 1 d . . . . . H15 H -0.005906 0.243863 0.676174 0.025 Uiso 1 1 calc R U . . . C21 C -0.15495(16) 0.12171(14) 0.69495(12) 0.0315(3) Uani 1 1 d . . . . . H34 H -0.101968 0.046936 0.661787 0.047 Uiso 1 1 calc R U . . . H35 H -0.234608 0.127537 0.642325 0.047 Uiso 1 1 calc R U . . . H36 H -0.199970 0.116116 0.753020 0.047 Uiso 1 1 calc R U . . . C22 C -0.12056(16) 0.35631(14) 0.79250(12) 0.0297(3) Uani 1 1 d . . . . . H37 H -0.163660 0.351477 0.851536 0.045 Uiso 1 1 calc R U . . . H38 H -0.201201 0.364551 0.741675 0.045 Uiso 1 1 calc R U . . . H39 H -0.046384 0.429170 0.819289 0.045 Uiso 1 1 calc R U . . . C23 C 0.16200(13) 0.45626(11) 0.68748(10) 0.0173(3) Uani 1 1 d . . . . . N3 N 0.04897(12) 0.47743(10) 0.62733(8) 0.0210(2) Uani 1 1 d . . . . . C24 C -0.00391(15) 0.59310(12) 0.66428(11) 0.0235(3) Uani 1 1 d . . . . . H1 H -0.085305 0.608234 0.621277 0.028 Uiso 1 1 calc R U . . . C25 C 0.05279(15) 0.68812(12) 0.75899(11) 0.0232(3) Uani 1 1 d . . . . . H2 H 0.013117 0.767481 0.779853 0.028 Uiso 1 1 calc R U . . . C26 C 0.17135(14) 0.66747(12) 0.82598(10) 0.0204(3) Uani 1 1 d . . . . . C27 C 0.23569(15) 0.76076(12) 0.92677(10) 0.0249(3) Uani 1 1 d . . . . . H3 H 0.200218 0.841799 0.951080 0.030 Uiso 1 1 calc R U . . . C28 C 0.34805(16) 0.73460(13) 0.98877(10) 0.0266(3) Uani 1 1 d . . . . . H4 H 0.389650 0.797435 1.056230 0.032 Uiso 1 1 calc R U . . . C29 C 0.40297(15) 0.61531(13) 0.95373(10) 0.0250(3) Uani 1 1 d . . . . . H5 H 0.480545 0.598120 0.998035 0.030 Uiso 1 1 calc R U . . . C30 C 0.34543(14) 0.52389(12) 0.85628(10) 0.0214(3) Uani 1 1 d . . . . . H6 H 0.384406 0.444174 0.832992 0.026 Uiso 1 1 calc R U . . . C31 C 0.22805(13) 0.54759(11) 0.78999(10) 0.0184(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0184(5) 0.0290(5) 0.0191(5) 0.0101(4) 0.0006(4) -0.0004(4) C1 0.0186(6) 0.0145(6) 0.0181(6) 0.0060(5) 0.0031(5) 0.0011(5) N1 0.0184(5) 0.0227(5) 0.0172(5) 0.0082(4) 0.0046(4) -0.0003(4) C2 0.0165(6) 0.0272(7) 0.0226(7) 0.0112(5) 0.0040(5) 0.0005(5) C3 0.0245(7) 0.0354(8) 0.0404(8) 0.0199(7) 0.0112(6) 0.0085(6) C4 0.0228(7) 0.0308(8) 0.0328(8) 0.0099(6) 0.0023(6) -0.0040(6) C5 0.0260(7) 0.0328(7) 0.0195(7) 0.0110(6) 0.0081(5) -0.0018(6) C6 0.0404(9) 0.0473(9) 0.0364(8) 0.0294(8) 0.0069(7) -0.0001(7) C7 0.0441(9) 0.0427(9) 0.0212(7) 0.0025(7) 0.0112(7) -0.0017(7) C8 0.0142(6) 0.0175(6) 0.0176(6) 0.0064(5) 0.0023(5) 0.0009(5) C9 0.0149(6) 0.0188(6) 0.0154(6) 0.0067(5) 0.0026(5) 0.0016(5) C10 0.0158(6) 0.0190(6) 0.0158(6) 0.0075(5) 0.0020(5) 0.0006(5) C11 0.0158(6) 0.0201(6) 0.0172(6) 0.0065(5) 0.0026(5) -0.0007(5) C12 0.0139(6) 0.0222(6) 0.0176(6) 0.0079(5) 0.0019(5) 0.0025(5) C13 0.0154(6) 0.0190(6) 0.0171(6) 0.0068(5) 0.0037(5) 0.0036(5) C14 0.0150(6) 0.0173(6) 0.0157(6) 0.0053(5) 0.0029(5) 0.0010(5) C15 0.0142(6) 0.0170(6) 0.0173(6) 0.0065(5) 0.0020(5) 0.0019(5) C16 0.0203(6) 0.0151(6) 0.0167(6) 0.0051(5) 0.0022(5) 0.0013(5) O2 0.0225(5) 0.0355(5) 0.0212(5) 0.0147(4) 0.0009(4) 0.0046(4) N2 0.0203(5) 0.0224(5) 0.0168(5) 0.0080(4) 0.0042(4) 0.0009(4) C17 0.0292(7) 0.0368(8) 0.0225(7) 0.0159(6) 0.0102(6) 0.0037(6) C18 0.0552(11) 0.0507(10) 0.0518(10) 0.0383(9) 0.0242(9) 0.0127(8) C19 0.0421(9) 0.0557(10) 0.0175(7) 0.0118(7) 0.0078(6) 0.0020(8) C20 0.0170(6) 0.0264(7) 0.0192(6) 0.0079(5) 0.0045(5) 0.0014(5) C21 0.0247(7) 0.0339(8) 0.0291(8) 0.0063(6) 0.0055(6) -0.0051(6) C22 0.0262(7) 0.0319(8) 0.0323(8) 0.0125(6) 0.0108(6) 0.0075(6) C23 0.0156(6) 0.0191(6) 0.0191(6) 0.0093(5) 0.0048(5) 0.0003(5) N3 0.0197(5) 0.0216(6) 0.0223(6) 0.0099(5) 0.0029(4) 0.0026(4) C24 0.0205(6) 0.0241(7) 0.0276(7) 0.0124(6) 0.0027(5) 0.0052(5) C25 0.0230(7) 0.0194(6) 0.0293(7) 0.0107(6) 0.0080(6) 0.0052(5) C26 0.0195(6) 0.0208(6) 0.0217(7) 0.0083(5) 0.0072(5) 0.0000(5) C27 0.0273(7) 0.0191(6) 0.0246(7) 0.0041(5) 0.0080(6) 0.0015(5) C28 0.0293(7) 0.0245(7) 0.0194(7) 0.0030(5) 0.0025(6) -0.0039(6) C29 0.0253(7) 0.0266(7) 0.0215(7) 0.0100(6) -0.0009(5) -0.0022(5) C30 0.0217(6) 0.0200(6) 0.0223(7) 0.0087(5) 0.0033(5) 0.0006(5) C31 0.0173(6) 0.0198(6) 0.0189(6) 0.0082(5) 0.0051(5) -0.0005(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 122.67(11) . . ? O1 C1 C8 117.96(11) . . ? N1 C1 C8 119.36(10) . . ? C1 N1 C2 122.99(10) . . ? C1 N1 C5 119.46(10) . . ? C2 N1 C5 117.54(10) . . ? N1 C2 C4 111.65(11) . . ? N1 C2 C3 111.55(11) . . ? C4 C2 C3 111.39(11) . . ? N1 C2 H12 107.3 . . ? C4 C2 H12 107.3 . . ? C3 C2 H12 107.3 . . ? C2 C3 H16 109.5 . . ? C2 C3 H17 109.5 . . ? H16 C3 H17 109.5 . . ? C2 C3 H18 109.5 . . ? H16 C3 H18 109.5 . . ? H17 C3 H18 109.5 . . ? C2 C4 H19 109.5 . . ? C2 C4 H20 109.5 . . ? H19 C4 H20 109.5 . . ? C2 C4 H21 109.5 . . ? H19 C4 H21 109.5 . . ? H20 C4 H21 109.5 . . ? N1 C5 C6 111.70(11) . . ? N1 C5 C7 112.04(11) . . ? C6 C5 C7 113.10(13) . . ? N1 C5 H13 106.5 . . ? C6 C5 H13 106.5 . . ? C7 C5 H13 106.5 . . ? C5 C6 H22 109.5 . . ? C5 C6 H23 109.5 . . ? H22 C6 H23 109.5 . . ? C5 C6 H24 109.5 . . ? H22 C6 H24 109.5 . . ? H23 C6 H24 109.5 . . ? C5 C7 H25 109.5 . . ? C5 C7 H26 109.5 . . ? H25 C7 H26 109.5 . . ? C5 C7 H27 109.5 . . ? H25 C7 H27 109.5 . . ? H26 C7 H27 109.5 . . ? C1 C8 C9 119.23(10) . . ? C1 C8 C13 124.29(10) . . ? C9 C8 C13 89.73(9) . . ? C1 C8 C11 132.82(10) . . ? C9 C8 C11 89.73(9) . . ? C13 C8 C11 89.07(9) . . ? C10 C9 C8 90.82(9) . . ? C10 C9 C14 90.83(9) . . ? C8 C9 C14 90.31(9) . . ? C10 C9 H7 124.8 . . ? C8 C9 H7 124.8 . . ? C14 C9 H7 124.8 . . ? C23 C10 C9 123.50(10) . . ? C23 C10 C11 122.45(10) . . ? C9 C10 C11 89.91(9) . . ? C23 C10 C15 130.62(10) . . ? C9 C10 C15 89.74(9) . . ? C11 C10 C15 88.98(9) . . ? C12 C11 C10 90.50(9) . . ? C12 C11 C8 90.41(9) . . ? C10 C11 C8 89.53(9) . . ? C12 C11 H8 125.2 . . ? C10 C11 H8 125.2 . . ? C8 C11 H8 125.2 . . ? C15 C12 C11 90.86(9) . . ? C15 C12 C13 90.28(9) . . ? C11 C12 C13 90.10(9) . . ? C15 C12 H9 125.0 . . ? C11 C12 H9 125.0 . . ? C13 C12 H9 125.0 . . ? C14 C13 C12 90.08(9) . . ? C14 C13 C8 89.65(9) . . ? C12 C13 C8 90.41(9) . . ? C14 C13 H10 125.2 . . ? C12 C13 H10 125.2 . . ? C8 C13 H10 125.2 . . ? C9 C14 C13 90.30(9) . . ? C9 C14 C15 90.61(9) . . ? C13 C14 C15 89.89(9) . . ? C9 C14 H11 125.1 . . ? C13 C14 H11 125.1 . . ? C15 C14 H11 125.1 . . ? C16 C15 C12 121.24(10) . . ? C16 C15 C14 124.88(10) . . ? C12 C15 C14 89.74(9) . . ? C16 C15 C10 130.72(10) . . ? C12 C15 C10 89.66(9) . . ? C14 C15 C10 88.81(9) . . ? O2 C16 N2 123.02(11) . . ? O2 C16 C15 118.56(11) . . ? N2 C16 C15 118.40(10) . . ? C16 N2 C20 123.10(10) . . ? C16 N2 C17 119.75(10) . . ? C20 N2 C17 117.15(10) . . ? N2 C17 C18 112.00(12) . . ? N2 C17 C19 111.22(11) . . ? C18 C17 C19 113.67(13) . . ? N2 C17 H14 106.5 . . ? C18 C17 H14 106.5 . . ? C19 C17 H14 106.5 . . ? C17 C18 H28 109.5 . . ? C17 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? C17 C18 H30 109.5 . . ? H28 C18 H30 109.5 . . ? H29 C18 H30 109.5 . . ? C17 C19 H31 109.5 . . ? C17 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? C17 C19 H33 109.5 . . ? H31 C19 H33 109.5 . . ? H32 C19 H33 109.5 . . ? N2 C20 C21 111.47(11) . . ? N2 C20 C22 112.17(11) . . ? C21 C20 C22 111.28(11) . . ? N2 C20 H15 107.2 . . ? C21 C20 H15 107.2 . . ? C22 C20 H15 107.2 . . ? C20 C21 H34 109.5 . . ? C20 C21 H35 109.5 . . ? H34 C21 H35 109.5 . . ? C20 C21 H36 109.5 . . ? H34 C21 H36 109.5 . . ? H35 C21 H36 109.5 . . ? C20 C22 H37 109.5 . . ? C20 C22 H38 109.5 . . ? H37 C22 H38 109.5 . . ? C20 C22 H39 109.5 . . ? H37 C22 H39 109.5 . . ? H38 C22 H39 109.5 . . ? N3 C23 C31 123.15(11) . . ? N3 C23 C10 115.28(11) . . ? C31 C23 C10 121.45(11) . . ? C23 N3 C24 117.95(11) . . ? C25 C24 N3 124.03(12) . . ? C25 C24 H1 118.0 . . ? N3 C24 H1 118.0 . . ? C24 C25 C26 119.32(12) . . ? C24 C25 H2 120.3 . . ? C26 C25 H2 120.3 . . ? C25 C26 C31 117.94(11) . . ? C25 C26 C27 123.05(12) . . ? C31 C26 C27 119.00(12) . . ? C28 C27 C26 120.40(12) . . ? C28 C27 H3 119.8 . . ? C26 C27 H3 119.8 . . ? C27 C28 C29 120.63(12) . . ? C27 C28 H4 119.7 . . ? C29 C28 H4 119.7 . . ? C30 C29 C28 120.53(12) . . ? C30 C29 H5 119.7 . . ? C28 C29 H5 119.7 . . ? C29 C30 C31 120.36(12) . . ? C29 C30 H6 119.8 . . ? C31 C30 H6 119.8 . . ? C30 C31 C26 119.07(11) . . ? C30 C31 C23 123.36(11) . . ? C26 C31 C23 117.57(11) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.2304(15) . ? C1 N1 1.3532(16) . ? C1 C8 1.5056(17) . ? N1 C2 1.4721(16) . ? N1 C5 1.4843(16) . ? C2 C4 1.5242(19) . ? C2 C3 1.5282(18) . ? C2 H12 1.0000 . ? C3 H16 0.9800 . ? C3 H17 0.9800 . ? C3 H18 0.9800 . ? C4 H19 0.9800 . ? C4 H20 0.9800 . ? C4 H21 0.9800 . ? C5 C6 1.516(2) . ? C5 C7 1.526(2) . ? C5 H13 1.0000 . ? C6 H22 0.9800 . ? C6 H23 0.9800 . ? C6 H24 0.9800 . ? C7 H25 0.9800 . ? C7 H26 0.9800 . ? C7 H27 0.9800 . ? C8 C9 1.5616(16) . ? C8 C13 1.5784(16) . ? C8 C11 1.5803(16) . ? C9 C10 1.5601(16) . ? C9 C14 1.5617(17) . ? C9 H7 1.0000 . ? C10 C23 1.4868(17) . ? C10 C11 1.5767(16) . ? C10 C15 1.6014(16) . ? C11 C12 1.5642(17) . ? C11 H8 1.0000 . ? C12 C15 1.5621(16) . ? C12 C13 1.5661(16) . ? C12 H9 1.0000 . ? C13 C14 1.5628(16) . ? C13 H10 1.0000 . ? C14 C15 1.5761(16) . ? C14 H11 1.0000 . ? C15 C16 1.5030(17) . ? C16 O2 1.2343(15) . ? C16 N2 1.3508(16) . ? N2 C20 1.4746(16) . ? N2 C17 1.4860(16) . ? C17 C18 1.521(2) . ? C17 C19 1.522(2) . ? C17 H14 1.0000 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C18 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C19 H33 0.9800 . ? C20 C21 1.5242(19) . ? C20 C22 1.5249(18) . ? C20 H15 1.0000 . ? C21 H34 0.9800 . ? C21 H35 0.9800 . ? C21 H36 0.9800 . ? C22 H37 0.9800 . ? C22 H38 0.9800 . ? C22 H39 0.9800 . ? C23 N3 1.3237(16) . ? C23 C31 1.4331(17) . ? N3 C24 1.3646(17) . ? C24 C25 1.3612(19) . ? C24 H1 0.9500 . ? C25 C26 1.4139(18) . ? C25 H2 0.9500 . ? C26 C31 1.4212(18) . ? C26 C27 1.4217(18) . ? C27 C28 1.364(2) . ? C27 H3 0.9500 . ? C28 C29 1.408(2) . ? C28 H4 0.9500 . ? C29 C30 1.3698(18) . ? C29 H5 0.9500 . ? C30 C31 1.4175(18) . ? C30 H6 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 N1 C2 -174.84(11) . . . . ? C8 C1 N1 C2 4.07(17) . . . . ? O1 C1 N1 C5 5.85(18) . . . . ? C8 C1 N1 C5 -175.24(11) . . . . ? C1 N1 C2 C4 -110.57(13) . . . . ? C5 N1 C2 C4 68.76(14) . . . . ? C1 N1 C2 C3 124.08(13) . . . . ? C5 N1 C2 C3 -56.59(15) . . . . ? C1 N1 C5 C6 58.61(16) . . . . ? C2 N1 C5 C6 -120.74(13) . . . . ? C1 N1 C5 C7 -69.46(15) . . . . ? C2 N1 C5 C7 111.19(13) . . . . ? O1 C1 C8 C9 -13.43(16) . . . . ? N1 C1 C8 C9 167.61(10) . . . . ? O1 C1 C8 C13 98.61(14) . . . . ? N1 C1 C8 C13 -80.35(15) . . . . ? O1 C1 C8 C11 -134.16(13) . . . . ? N1 C1 C8 C11 46.88(18) . . . . ? C1 C8 C9 C10 -139.81(11) . . . . ? C13 C8 C9 C10 90.17(9) . . . . ? C11 C8 C9 C10 1.09(9) . . . . ? C1 C8 C9 C14 129.35(11) . . . . ? C13 C8 C9 C14 -0.67(9) . . . . ? C11 C8 C9 C14 -89.74(9) . . . . ? C8 C9 C10 C23 128.88(11) . . . . ? C14 C9 C10 C23 -140.80(11) . . . . ? C8 C9 C10 C11 -1.10(9) . . . . ? C14 C9 C10 C11 89.22(9) . . . . ? C8 C9 C10 C15 -90.07(9) . . . . ? C14 C9 C10 C15 0.25(8) . . . . ? C23 C10 C11 C12 139.90(11) . . . . ? C9 C10 C11 C12 -89.33(9) . . . . ? C15 C10 C11 C12 0.41(9) . . . . ? C23 C10 C11 C8 -129.69(11) . . . . ? C9 C10 C11 C8 1.08(9) . . . . ? C15 C10 C11 C8 90.82(9) . . . . ? C1 C8 C11 C12 -139.19(13) . . . . ? C9 C8 C11 C12 89.41(9) . . . . ? C13 C8 C11 C12 -0.33(8) . . . . ? C1 C8 C11 C10 130.31(13) . . . . ? C9 C8 C11 C10 -1.08(9) . . . . ? C13 C8 C11 C10 -90.82(9) . . . . ? C10 C11 C12 C15 -0.42(9) . . . . ? C8 C11 C12 C15 -89.95(9) . . . . ? C10 C11 C12 C13 89.86(9) . . . . ? C8 C11 C12 C13 0.33(8) . . . . ? C15 C12 C13 C14 0.88(9) . . . . ? C11 C12 C13 C14 -89.98(9) . . . . ? C15 C12 C13 C8 90.53(9) . . . . ? C11 C12 C13 C8 -0.33(8) . . . . ? C1 C8 C13 C14 -125.34(11) . . . . ? C9 C8 C13 C14 0.67(9) . . . . ? C11 C8 C13 C14 90.40(8) . . . . ? C1 C8 C13 C12 144.59(11) . . . . ? C9 C8 C13 C12 -89.40(9) . . . . ? C11 C8 C13 C12 0.33(8) . . . . ? C10 C9 C14 C13 -90.14(9) . . . . ? C8 C9 C14 C13 0.68(9) . . . . ? C10 C9 C14 C15 -0.25(9) . . . . ? C8 C9 C14 C15 90.57(9) . . . . ? C12 C13 C14 C9 89.74(9) . . . . ? C8 C13 C14 C9 -0.67(9) . . . . ? C12 C13 C14 C15 -0.87(9) . . . . ? C8 C13 C14 C15 -91.28(9) . . . . ? C11 C12 C15 C16 -139.00(11) . . . . ? C13 C12 C15 C16 130.89(11) . . . . ? C11 C12 C15 C14 89.23(9) . . . . ? C13 C12 C15 C14 -0.87(9) . . . . ? C11 C12 C15 C10 0.42(9) . . . . ? C13 C12 C15 C10 -89.68(9) . . . . ? C9 C14 C15 C16 141.60(11) . . . . ? C13 C14 C15 C16 -128.10(11) . . . . ? C9 C14 C15 C12 -89.43(9) . . . . ? C13 C14 C15 C12 0.87(9) . . . . ? C9 C14 C15 C10 0.24(8) . . . . ? C13 C14 C15 C10 90.54(9) . . . . ? C23 C10 C15 C16 -1.4(2) . . . . ? C9 C10 C15 C16 -137.71(12) . . . . ? C11 C10 C15 C16 132.37(13) . . . . ? C23 C10 C15 C12 -134.18(13) . . . . ? C9 C10 C15 C12 89.50(9) . . . . ? C11 C10 C15 C12 -0.41(9) . . . . ? C23 C10 C15 C14 136.07(13) . . . . ? C9 C10 C15 C14 -0.24(8) . . . . ? C11 C10 C15 C14 -90.16(8) . . . . ? C12 C15 C16 O2 2.08(17) . . . . ? C14 C15 C16 O2 116.69(13) . . . . ? C10 C15 C16 O2 -118.79(14) . . . . ? C12 C15 C16 N2 -176.15(10) . . . . ? C14 C15 C16 N2 -61.55(16) . . . . ? C10 C15 C16 N2 62.98(17) . . . . ? O2 C16 N2 C20 179.62(11) . . . . ? C15 C16 N2 C20 -2.23(17) . . . . ? O2 C16 N2 C17 -0.52(18) . . . . ? C15 C16 N2 C17 177.63(11) . . . . ? C16 N2 C17 C18 -63.49(16) . . . . ? C20 N2 C17 C18 116.38(14) . . . . ? C16 N2 C17 C19 64.93(16) . . . . ? C20 N2 C17 C19 -115.20(13) . . . . ? C16 N2 C20 C21 115.97(13) . . . . ? C17 N2 C20 C21 -63.89(14) . . . . ? C16 N2 C20 C22 -118.48(13) . . . . ? C17 N2 C20 C22 61.66(15) . . . . ? C9 C10 C23 N3 -4.33(17) . . . . ? C11 C10 C23 N3 110.42(13) . . . . ? C15 C10 C23 N3 -128.41(13) . . . . ? C9 C10 C23 C31 179.46(10) . . . . ? C11 C10 C23 C31 -65.79(16) . . . . ? C15 C10 C23 C31 55.38(18) . . . . ? C31 C23 N3 C24 1.68(18) . . . . ? C10 C23 N3 C24 -174.46(11) . . . . ? C23 N3 C24 C25 0.25(19) . . . . ? N3 C24 C25 C26 -1.6(2) . . . . ? C24 C25 C26 C31 1.04(18) . . . . ? C24 C25 C26 C27 -179.04(12) . . . . ? C25 C26 C27 C28 178.77(13) . . . . ? C31 C26 C27 C28 -1.32(19) . . . . ? C26 C27 C28 C29 0.5(2) . . . . ? C27 C28 C29 C30 0.6(2) . . . . ? C28 C29 C30 C31 -1.0(2) . . . . ? C29 C30 C31 C26 0.15(18) . . . . ? C29 C30 C31 C23 -179.64(12) . . . . ? C25 C26 C31 C30 -179.10(11) . . . . ? C27 C26 C31 C30 0.98(18) . . . . ? C25 C26 C31 C23 0.71(17) . . . . ? C27 C26 C31 C23 -179.21(11) . . . . ? N3 C23 C31 C30 177.65(12) . . . . ? C10 C23 C31 C30 -6.44(18) . . . . ? N3 C23 C31 C26 -2.15(18) . . . . ? C10 C23 C31 C26 173.76(11) . . . . ?